CN110423916B - Silicon dioxide aerogel loaded copper-based composite material and preparation method thereof - Google Patents
Silicon dioxide aerogel loaded copper-based composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a silicon dioxide aerogel loaded copper-based composite material and a preparation method thereof. The invention adopts sol-gel method, belongs to molecular level compounding, and adopts vacuum hot-pressing sintering, thus achieving the purposes of uniform dispersed phase distribution, high density and excellent material comprehensive performance, and meeting the requirements of devices such as switch contact bridges of electrical engineering, integrated circuit lead frames, overhead conductor cores of high-speed railway electric locomotives and the like.
Description
Technical Field
The invention belongs to the field of preparation of composite materials. In particular to a silicon dioxide aerogel loaded copper-based composite material and a preparation method thereof.
Background
The conductivity, the electric heating property and the melting point of copper are all close to those of silver, but the high-temperature strength of copper is lower, and the defects of easy abrasion, poor arc corrosion resistance and the like exist in the using process. The copper-based composite material prepared by adding the reinforcement into the copper matrix not only maintains the advantages of high electrical conductivity, high thermal conductivity, good ductility and the like of copper, but also makes up the defects of low hardness and yield strength, poor fusion welding resistance and the like of copper, so that the copper-based composite material is widely applied to various fields of electric power, electrician, mechanical manufacturing and the like.
In order to improve the mechanical properties of the copper-based composite material at room temperature and high temperature and simultaneously keep the excellent physical properties of the copper material, a reinforcement introduced into a copper matrix must have good chemical stability at high temperature, and no obvious structural and performance changes occur in the preparation and use processes of the copper-based composite material. Currently, common reinforcement materials are: (1) fiber reinforcements such as alumina fibers, carbon fibers, or boron fibers; (2) oxide (Al)2O3、BeO2、SiO2) Whisker, non-oxide (SiC, N)4) Whisker reinforcements such as whiskers and metal (e.g., Cu, Fe, Ni, Cr, etc.) whiskers; (3) oxides, carbides, nitrides, borides (e.g. Al)2O3、ZrO2SiC, etc.) ceramic-based particle reinforcement and graphite, intermetallicCompound (FeAl, MoSi)2Etc.), a particulate reinforcement of a metallic material (W, Mo, etc.).
At present, the most common commercial production of copper-based composite materials at home and abroad is the alumina dispersion strengthening copper-based composite material, and the process mainly adopts an internal oxygen method and a mechanical alloying method. However, the internal oxidation method has complex process, long cycle, high cost, difficult control of oxygen amount and oxidation time, extremely strict requirements on equipment and process control, and simultaneously, oxidant retained in the copper-based composite material is difficult to completely eliminate, thus easily causing structural defects such as cracks, cavities, impurities and the like to generate certain influence on the performance of the material. The mechanical alloying method is limited by the disadvantages that the grain size of the strengthening phase is not fine enough, the grain size distribution is wide, impurities are easy to be mixed in, and uniform mixing is difficult.
The aerogel is a novel light nano porous amorphous solid material with a controllable structure, the typical size of the pore diameter is 1-100nm, and the specific surface area is up to 200-2The copper-based composite material is a novel material with a wide application prospect and a plurality of unique properties, and the unique nano porous structure enables the silicon dioxide aerogel to become a very ideal carrier of nano particles, copper is loaded on the carrier to serve as a reinforcement of the copper-based composite material, and the copper loaded on the aerogel can prevent the aerogel from being agglomerated. Currently, silica aerogels are mostly used for catalysis and adsorption. According to the invention, the silicon dioxide aerogel loaded copper is used for the reinforcement of the copper-based composite material for the first time and can be dispersedly distributed in the copper matrix.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a silicon dioxide aerogel loaded copper-based composite material and a preparation method thereof, which can be used for preparing the copper-based composite material with uniformly distributed dispersed phases, high density and excellent comprehensive performance, and can be used for industrial production, and the process is simple and the production efficiency is high.
In order to solve the technical problems, the technical solution of the invention is as follows:
the invention provides a silicon dioxide aerogel supported copper-based composite material, which comprises the components and the weight percentageThe content of each component is as follows: SiO 220.5-4%, and the balance of Cu.
Further, the silica particles have an average particle size of 50 to 200 nm.
The invention also provides a preparation method of the silicon dioxide aerogel loaded copper-based composite material, which takes soluble copper salt, ethyl orthosilicate and citric acid as raw materials, and prepares according to mixed solution → sol-gel preparation → freeze drying or vacuum drying → calcining → grinding → reduction → vacuum hot pressing and sintering → the silicon dioxide aerogel loaded copper-based composite material is obtained.
Further, the specific steps are as follows:
firstly, dissolving copper nitrate trihydrate, ethyl orthosilicate and citric acid in deionized water according to a proportion to obtain a clear solution;
secondly, heating the solution in a magnetic stirrer to be stirred to obtain viscous mixed gel;
step three, carrying out freeze drying or vacuum drying on the gel obtained in the step two to obtain blue spongy substances with different fluffy amounts;
fourthly, calcining the blue fluffy object obtained after drying at a certain temperature to obtain fluffy black composite material of silica aerogel and copper oxide;
fifthly, grinding the fluffy black composite substance obtained in the fourth step into powder in a bowl mill to obtain silicon dioxide-copper oxide black composite powder;
sixthly, putting the black composite powder obtained in the fifth step in hydrogen atmosphere to obtain silicon oxide aerogel-copper composite powder;
step seven, putting the composite powder obtained in the step six into a sintering mold for vacuum hot-pressing sintering;
further, in the second step, the heating temperature was 80 ℃.
Further, in the fourth step, the calcination temperature is 600-700 ℃, and the calcination time is 6-7 hours.
Further, in the sixth step, the reduction condition is that the reduction temperature is 400-500 ℃ and the reduction time is 2-3 hours.
Further, in the seventh step, the vacuum hot-pressing sintering is carried out, wherein the temperature is raised to 500-600 ℃ at the temperature rise rate of 10-15 ℃/min, and the temperature is kept for 30-40 min; continuously heating to 900-1000 deg.C at a temperature rise rate of 5-10 deg.C/min, loading 30-40MPa pressure, maintaining the temperature and pressure for 60-80min, and cooling with the furnace.
After the scheme is adopted, the invention has the beneficial effects that: (1) the process is simple, the production efficiency is high, and the method can be applied to industrial production; (2) all raw materials are mixed among liquid phase molecules, so that the copper-based composite material with uniformly distributed dispersed phases can be obtained; (3) vacuum hot-pressing sintering is adopted, and the product can obtain high compactness degree and good comprehensive performance without extrusion or re-pressing and re-sintering processes.
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FIG. 1 is a flow chart of a preparation method in an embodiment of the present invention.
Detailed Description
The technical solutions of the present invention are further described below with reference to the accompanying drawings, and the following descriptions are only used for understanding the present invention and are not used to limit the scope of the present invention.
The silicon dioxide aerogel load copper-based composite material provided by the invention comprises the following components in percentage by weight: SiO 220.5-4%, and the balance of Cu. Further, the silica particles have an average particle size of 50 to 200 nm.
As shown in FIG. 1, the preparation process of the present invention in the following examples was carried out according to the scheme shown in FIG. 1. Soluble copper salt, tetraethoxysilane and citric acid are used as raw materials, and the silicon dioxide aerogel supported copper-based composite material is obtained according to the steps of mixed solution preparation → sol gel preparation → freeze drying or vacuum drying → calcination → grinding → reduction → vacuum hot pressing and sintering → the obtained product is obtained.
Further, the specific steps are as follows:
firstly, dissolving copper nitrate trihydrate, ethyl orthosilicate and citric acid in deionized water according to a proportion to obtain a clear solution;
secondly, heating the solution in a magnetic stirrer to 80 ℃ and stirring to obtain viscous mixed gel;
step three, freeze drying or vacuum drying the gel obtained in the step two to obtain blue spongy substances with different fluffy amounts; all the raw materials in the sol-gel method belong to molecular level mixing due to solution mixing, so that the reinforced phase can be dispersed and uniformly distributed, and the silicon dioxide aerogel can be uniformly dispersed and distributed in the copper matrix.
Fourthly, calcining the blue fluffy object obtained after drying at a certain temperature to obtain fluffy black composite material of silica aerogel and copper oxide;
fifthly, grinding the fluffy black composite substance obtained in the sixth step into powder in a bowl mill to obtain silicon dioxide-copper oxide black composite powder;
sixthly, reducing the black composite powder obtained in the fifth step for a period in a hydrogen atmosphere at a certain temperature to obtain silicon oxide aerogel-copper composite powder;
step seven, putting the composite powder obtained in the step six into a sintering mold for vacuum hot-pressing sintering;
further, in the second step, the heating temperature is 80 ℃, in the fourth step, the calcination temperature is 600-700 ℃, the calcination time is 6-7 hours, so as to fully decompose the compound, in the sixth step, the reduction condition is 400-500 ℃, the reduction time is 2-3 hours, in the seventh step, the vacuum hot-pressing sintering is carried out, wherein the temperature rise rate is increased to 500-600 ℃ at a speed of 10-15 ℃/min, and the constant temperature is 30-40 minutes; continuously heating to 900-1000 deg.C at a temperature rise rate of 5-10 deg.C/min, loading 30-40MPa pressure, maintaining the temperature and pressure for 60-80min, and cooling with the furnace.
The first embodiment is as follows: with Cu-0.5SiO2Composite materials are exemplified
1. Weighing 2.4g of copper nitrate trihydrate and 2.1g of citric acid monohydrate, dissolving in a proper amount of deionized water to obtain a clear solution, then dropwise adding 0.03ml of ethyl orthosilicate into the clear solution, continuously stirring the mixed solution in a magnetic stirrer, controlling the water bath temperature at 80 ℃, and continuously stirring until the mixed solution becomes viscous gel.
2. The gels were dried in a freeze-drying oven at 80 ℃ to give a blue, fluffy sponge-like material.
3. And (3) calcining the dried blue spongy substance in a muffle furnace at the temperature of 600 ℃ for 6 hours to obtain the fluffy black composite substance of the silica aerogel loaded with the copper oxide. And grinding the fluffy black composite substance in a grinding bowl to obtain the black composite powder of the silica aerogel loaded with the copper oxide.
4. Carrying out hydrogen reduction on the black composite powder in a tubular furnace, wherein the reduction temperature is 400 ℃, and the reduction time is 3 hours to obtain silicon dioxide aerogel copper-loaded composite powder;
5. loading the obtained reduction composite powder into a sintering mold for vacuum hot-pressing sintering, raising the temperature to 500 ℃ at a heating rate of 15 ℃/min, and keeping the temperature for 30 min; continuously increasing the temperature to 900 ℃ at the heating rate of 10 ℃/min, loading the pressure of 30MPa, keeping the temperature and the pressure for 60min, and then cooling along with the furnace.
The properties of the material obtained in this example were: resistivity: 2.75 mu omega cm; hardness: 87 (HV); density: 7.6g/cm3；SiO2The average particle size of the particles was 60 nm.
Example two: with Cu-1SiO2Composite materials are exemplified
1. Weighing 2.4g of copper nitrate trihydrate and 2.1g of citric acid monohydrate, dissolving in a proper amount of deionized water to obtain a clear solution, then dropwise adding 0.06ml of tetraethoxysilane into the clear solution, continuously stirring the mixed solution in a magnetic stirrer, controlling the water bath temperature at 80 ℃, and continuously stirring until the mixed solution becomes viscous gel.
2. The gels were dried in vacuum drying ovens at 80 ℃ to give blue fluffy sponge-like materials.
3. And (3) calcining the dried blue spongy substance in a muffle furnace at the temperature of 650 ℃ for 6 hours to obtain the fluffy black composite substance of the silica aerogel loaded with the copper oxide. And grinding the fluffy black composite substance in a grinding bowl to obtain the black composite powder of the silica aerogel loaded with the copper oxide.
4. Carrying out hydrogen reduction on the black composite powder in a tubular furnace, wherein the reduction temperature is 400 ℃, and the reduction time is 3 hours to obtain silicon dioxide aerogel copper-loaded composite powder;
5. loading the obtained reduction composite powder into a sintering mold for vacuum hot-pressing sintering, raising the temperature to 500 ℃ at a heating rate of 15 ℃/min, and keeping the temperature for 30 min; continuously increasing the temperature to 950 ℃ at the heating rate of 10 ℃/min, loading the pressure of 30MPa, keeping the temperature and the pressure for 60min, and then cooling along with the furnace.
The properties of the material obtained in this example were: conductivity: 2.81 μ Ω. cm; hardness: 90 (HV); density: 7.55g/cm3；SiO2The average particle size of the particles was 70 nm.
Example three: with Cu-2SiO2Composite materials are exemplified
1. Weighing 4.8g of copper nitrate trihydrate and 4.2g of citric acid monohydrate, dissolving in a proper amount of deionized water to obtain a clear solution, then dropwise adding 0.36ml of ethyl orthosilicate into the clear solution, continuously stirring the mixed solution in a magnetic stirrer, controlling the water bath temperature at 80 ℃, and continuously stirring until the mixed solution becomes viscous gel.
2. The gels were dried in a freeze-drying oven at 80 ℃ to give a blue, fluffy sponge-like material.
3. And (3) calcining the dried blue spongy substance in a muffle furnace at the temperature of 600 ℃ for 6 hours to obtain the fluffy black composite substance of the silica aerogel loaded with the copper oxide. And grinding the fluffy black composite substance in a grinding bowl to obtain the black composite powder of the silica aerogel loaded with the copper oxide.
4. Carrying out hydrogen reduction on the black composite powder in a tubular furnace, wherein the reduction temperature is 400 ℃, and the reduction time is 3 hours to obtain silicon dioxide aerogel copper-loaded composite powder;
5. loading the obtained reduction composite powder into a sintering mold for vacuum hot-pressing sintering, raising the temperature to 600 ℃ at a heating rate of 15 ℃/min, and keeping the temperature for 30 min; continuously heating to 1000 ℃ at the heating rate of 10 ℃/min, loading the pressure of 30MPa, keeping the temperature and the pressure for 60min, and then cooling along with the furnace.
The properties of the material obtained in this example were: resistivity: 2.86 μ Ω. cm; hardness: 92 (HV); density:7.5g/cm3；SiO2the average particle size of the particles is: 100 nm.
Example four: with Cu-3SiO2Composite materials are exemplified
1. Weighing 7.2g of copper nitrate trihydrate and 6.3g of citric acid monohydrate, dissolving in a proper amount of deionized water to obtain a clear solution, then dropwise adding 0.83ml of ethyl orthosilicate into the clear solution, continuously stirring the mixed solution in a magnetic stirrer, controlling the water bath temperature at 80 ℃, and continuously stirring until the mixed solution becomes viscous gel.
2. The gels were dried in vacuum drying ovens at 80 ℃ to give blue fluffy sponge-like materials.
3. And (3) calcining the dried blue spongy substance in a muffle furnace at the temperature of 650 ℃ for 6 hours to obtain the fluffy black composite substance of the silica aerogel loaded with the copper oxide. And grinding the fluffy black composite substance in a grinding bowl to obtain the black composite powder of the silica aerogel loaded with the copper oxide.
4. Carrying out hydrogen reduction on the black composite powder in a tubular furnace, wherein the reduction temperature is 400 ℃, and the reduction time is 3 hours to obtain silicon dioxide aerogel copper-loaded composite powder;
5. loading the obtained reduction composite powder into a sintering mold for vacuum hot-pressing sintering, raising the temperature to 600 ℃ at a heating rate of 15 ℃/min, and keeping the temperature for 30 min; continuously heating to 1000 ℃ at the heating rate of 10 ℃/min, loading the pressure of 30MPa, keeping the temperature and the pressure for 60min, and then cooling along with the furnace.
The properties of the material obtained in this example were: resistivity: 2.9 mu omega cm; hardness: 95 (HV); density: 7.55g/cm3；SiO2The average particle size of the particles was 80 nm.
Example five: with Cu-4SiO2Composite materials are exemplified
1. Weighing 7.2g of copper nitrate trihydrate and 6.3g of citric acid monohydrate, dissolving in a proper amount of deionized water to obtain a clear solution, then dropwise adding 1.1ml of ethyl orthosilicate into the clear solution, continuously stirring the mixed solution in a magnetic stirrer, controlling the water bath temperature at 80 ℃, and continuously stirring until the mixed solution becomes viscous gel.
2. The gels were dried in vacuum drying ovens at 80 ℃ to give blue fluffy sponge-like materials.
3. And (3) calcining the dried blue spongy substance in a muffle furnace at the temperature of 600 ℃ for 6 hours to obtain the fluffy black composite substance of the silica aerogel loaded with the copper oxide. And grinding the fluffy black composite substance in a grinding bowl to obtain the black composite powder of the silica aerogel loaded with the copper oxide.
4. Carrying out hydrogen reduction on the black composite powder in a tubular furnace, wherein the reduction temperature is 400 ℃, and the reduction time is 3 hours to obtain silicon dioxide aerogel copper-loaded composite powder;
5. loading the obtained reduction composite powder into a sintering mold for vacuum hot-pressing sintering, raising the temperature to 500 ℃ at a heating rate of 15 ℃/min, and keeping the temperature for 30 min; continuously increasing the temperature to 900 ℃ at the heating rate of 10 ℃/min, loading the pressure of 30MPa, keeping the temperature and the pressure for 60min, and then cooling along with the furnace.
The properties of the material obtained in this example were: resistivity: 3.1 μ Ω. cm; hardness: 93 (HV); density: 7.6g/cm3；SiO2The average particle size of the particles was 120 nm.
The silicon dioxide aerogel load copper-based composite material prepared by the method can be applied to the high and new technical fields of electronic information, high-speed electric railway overhead lines, resistance welding electrodes of automobiles, high-thrust rocket engine linings and the like, and is widely applicable.
Claims (7)
1. The preparation method of the silicon dioxide aerogel loaded copper-based composite material is characterized by comprising the following steps of: soluble copper salt, tetraethoxysilane and citric acid are taken as raw materials, and the silicon dioxide aerogel load copper-based composite material is obtained according to the steps of mixed solution preparation → sol gel preparation → freeze drying or vacuum drying → calcination → grinding → reduction → vacuum hot pressing and sintering → the concrete steps are as follows: firstly, dissolving copper nitrate trihydrate, ethyl orthosilicate and citric acid in deionized water according to a proportion to obtain a clear solution; secondly, heating the solution in a magnetic stirrer to be stirred to obtain viscous mixed gel; step three, carrying out freeze drying or vacuum drying on the gel obtained in the step two to obtain blue spongy substances with different fluffy amounts; fourthly, calcining the blue fluffy object obtained after drying at a certain temperature to obtain fluffy black composite material of silica aerogel and copper oxide; fifthly, grinding the fluffy black composite substance obtained in the fourth step into powder in a bowl mill to obtain silicon dioxide-copper oxide black composite powder; sixthly, reducing the black composite powder obtained in the fifth step in a hydrogen atmosphere to obtain silicon oxide aerogel-copper composite powder; and step seven, filling the composite powder obtained in the step six into a sintering mold for vacuum hot-pressing sintering.
2. The method for preparing a silica aerogel-supported copper-based composite material as claimed in claim 1, wherein, in the second step, the heating temperature is 80 ℃.
3. The method for preparing the silica aerogel supported copper-based composite material as claimed in claim 1, wherein in the fourth step, the calcination temperature is 600-700 ℃ and the calcination time is 6-7 hours.
4. The method for preparing the silica aerogel-supported copper-based composite material as claimed in claim 1, wherein in the sixth step, the reduction conditions are 400-500 ℃ at the reduction temperature for 2-3 hours.
5. The preparation method of the silica aerogel supported copper-based composite material as claimed in claim 1, wherein in the seventh step, the vacuum hot-pressing sintering is performed, wherein the temperature is raised to 500-600 ℃ at a heating rate of 10-15 ℃/min, and the temperature is kept for 30-40 min; continuously heating to 900-1000 deg.C at a temperature rise rate of 5-10 deg.C/min, loading 30-40MPa pressure, maintaining the temperature and pressure for 60-80min, and cooling with the furnace.
6. A silica aerogel-supported copper-based composite prepared by the method of claim 1, wherein: comprisesComprises the following components in percentage by weight: SiO 220.5-4%, and the balance of Cu.
7. The silica aerogel-supported copper-based composite material of claim 6, wherein said SiO is2The average particle size of the particles is 50-200 nm.
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